CN106498464A - A kind of metal receives a micron preparation method for dendrite oldered array - Google Patents
A kind of metal receives a micron preparation method for dendrite oldered array Download PDFInfo
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Abstract
The invention discloses a kind of metal receives a micron preparation method for dendrite oldered array, with conductive array substrate as working electrode, electrolyte includes that metal salt solution and consumption are additive of the metal salt solution by molar concentration meter 0～5%, a micron dendrite is received in the controllable electrodeposit metals in its surface by voltammetry, obtain metal and receive a micron dendrite oldered array, the conductive array substrate is the substrate with orderly conductive array, the additive includes chelating agent or at least one in surfactant, and which is used for the formation for promoting metal to receive micron dendrite and regulates and controls pattern.The metal that the present invention is provided receives a micron preparation method for dendrite oldered array, process is simple, it is easy to operate, and Production Time is short, efficiency high, it is adaptable to which industrialized production and application, obtained metallic dendrite oldered array shape, thickness, size are controllable.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of metal receives a micron preparation side for dendrite oldered array
Method.
Background technology
Metal receives micron dendrite oldered array because which is widely applied prospect, the heat that always studies in recent decades
Door.An its very important application is from the regulation and control of primitive and based on the chemical and biological of the mechanism to metal surface etc.
Molecule sensing technology.Metallic dendrite array structure can achieve high throughput chemical and biomolecule sensing.In addition metallic dendrite array
The aspects such as the fields such as catalysis and the fuel cell of chemical reaction can also be can be applicable to.Traditional metal receive micron dendrite preparation not
Only it is difficult to make which in order, and uncontrollable metal receives the features such as the shape of micron dendrite, size, thickness.These factors are limited
Metal receives the application of micron dendrite.
At present, also there is no can to receive the method for micron dendrite oldered array growth with the control metal of system.
Content of the invention
Present invention aim to address the problems referred to above, there is provided a kind of simple to operation, size is controllable, efficiency high metal is received
The preparation method of micron dendrite oldered array.
For solving above-mentioned technical problem, the technical scheme is that：A kind of metal receives a micron system for dendrite oldered array
Preparation Method, with conductive array substrate as working electrode, electrolyte includes metal salt solution and consumption and massages for metal salt solution
The additive of your densitometer 0～5%, receives a micron dendrite by voltammetry in the controllable electrodeposit metals in its surface, obtains metal and receive
Micron dendrite oldered array, the conductive array substrate is the substrate with orderly conductive array, and the additive includes complexation
At least one in agent EDTA or surfactant, its are used for the formation for promoting metal to receive micron dendrite and regulate and control pattern.
In above-mentioned technical proposal, it is to make metal receive micron using the purpose of the conductive array substrate with orderly conductive array
Dendrite ordered arrangement and growth.For reaching above-mentioned purpose, can adopt but be not limited to photoetching process, microcontact printing techniques
In (Microcontact Printing, μ CP) or dip-pen nano process technology (Dip-pen lithography, DPN)
A kind of method prepares conductive array substrate.Every under the guiding theory of the present invention, prepare in order conduction battle array commonly used in the art
Other preparation methoies that chooses in row method fall within protection scope of the present invention.Microcontact printing techniques first pass through optics or electricity
Beamlet is lithographically derived template, and the precursor of polydimethylsiloxane (PDMS) die material solidifies in a template, polymerization forming
Depart from from template afterwards, just obtained carrying out the pressing mold required by micro-contact printing, then, PDMS pressing molds are immersed in black solution,
Then the pressing mold of dipped ink is pressed onto on substrate and can be prepared by required conductive array pattern, PDMS seals can repeatedly soak ink to be repeated to make
With.Dip-pen nano processing lithographic technique passes through to being transferred material precise control, can be existed by atomic-force microscope needle-tip
Substrate surface constructs arbitrary nanostructured.In the present invention, it is preferred to photoetching process prepares conductive array substrate.Photoetching process
Other existing methods for preparing conductive array substrate are compared, simple to operate, process is easy to control.
In above-mentioned technical proposal, conductive array substrate is prepared based on photoetching process, following steps are specifically included：
S1, prepares conductive array substrate：Photoresist is uniformly coated to substrate, coating thickness is 0.1～20 μm, is placed in
Toast after irradiating under ultraviolet light, the conductive array substrate with orderly conductive array is obtained；
S2, prepares metal and receives a micron dendrite oldered array：With conductive array substrate obtained in S1 as working electrode, electrolyte
It is the additive that metal salt solution presses molar concentration meter 0～5% including metal salt solution and consumption, by voltammetry on its surface
Controllable electrodeposit metals receive a micron dendrite, obtain metal and receive a micron dendrite oldered array.
In above-mentioned technical proposal, substrate is that the substrate can be selected but not limited as the carrier for preparing orderly conductive array
In N-type semiconductor or metal spraying conductor.Actually all chemically inert conductive substrates are suitable for the preparation method of present invention offer
Substrate can be done.Every the present invention thought guidance under, in substrate commonly used in the art or substrate choose other substrates or lining
Bottom falls within protection scope of the present invention.
In above-mentioned technical proposal, the ultraviolet wavelength in photoetching process, irradiation time, irradiation temperature, baking temperature, baking
The parameters such as roasting time can adopt routine, be not particularly limited, and its purpose is to obtain conduction battle array in order in substrate
Row.According to the research of inventor, ultraviolet wavelength is 200-400nm, and irradiation time is 2-300s, and irradiation temperature is 40-200
DEG C, good exposure effect can be reached；Baking temperature is 60-240 DEG C, when baking time is 10-60min, finally can obtain
Obtain the good conductive array substrate of combination property.
In above-mentioned technical proposal, photoresist in the conductive bore dia of orderly conductive array and pitch of holes, and photoetching process
Coating thickness, can directly affect and subsequently prepare metal and receive the growth and formation of micron dendrite.Studied according to inventor, for
The most metals such as copper, silver, gold, platinum, palladium, the conductive hole of orderly conductive array are a diameter of 0.1～10 μm, and conductive pitch of holes is one
To between 100 μm, photoresist coating thickness is 0.1～20 μm, can form high-sequential well-crystallized in individual conductive hole aperture
Metallic dendrite array.
In above-mentioned technical proposal, electro-deposition operating process, voltage need to according to material category, floor parameter, Arrays Aluminum Films in Acid Solution,
The parametric synthesis such as concentration, additive consider.The size of applied voltage directly affects whether can generate metallic dendrite structure, to not
When same metal forms pine-tree structure, the size of applied voltage is different, needs to be joined according to Arrays Aluminum Films in Acid Solution, concentration and substrate
Number synthesis consider.Voltage changes the appearance structure that can also regulate and control metallic dendrite.The big I of metallic dendrite is added by sedimentation time
To control.According to the research of inventor, applied voltage is -5～10V, and electrodeposition time can be set according to applied voltage and finally
The size of fixed metallic dendrite is confirming.Electrodeposition time in the present invention is 10s～10h.Complete in electro-deposition operation
Afterwards, conductive array substrate is removed, natural air drying is dried and obtains metal and receive a micron dendrite oldered array.Metal receives a micron dendrite
For metal dendritic structure, size is between 10nm～100 μm.
In above-mentioned technical proposal, the purpose of additive is to promote the formation of metallic dendrite and regulate and control pattern.Additive
At least one including but not limited in the additive such as surfactant, chelating agent, also includes the additives such as pH buffer.
Every other additives that under the thought guidance of the present invention, chooses in the additive for promoting dendrite to be formed commonly used in the art
Belong to protection scope of the present invention.Some metal salt solutions such as silver nitrate and chlorauric acid solution, can directly form without the need for additive
Pine-tree structure, in some metal salt solutions such as in the solution such as Palladous chloride., copper nitrate, rationally can add pH buffer, chelating agent or
The additives such as surfactant are promoting the formation of dendrite.It should be noted that with regard to specifically selecting which kind of surfactant, pH
Buffer agent or chelating agent, can be selected according to practical situation, such as chelating agent：Tetraacethyl diamino-vinyl (EDTA), surface are lived
Property agent：Cetyl trimethylammonium bromide (CTAB), dodecylbenzene sodium sulfonate (SDS), polyvinylpyrrolidone (PVP) etc..
Processed based on microcontact printing techniques (Microcontact Printing, μ CP) or dip-pen nano in the present invention
Technology (Dip-pen lithography, DPN) prepares the metal of conductive array substrate and receives a micron dendrite oldered array, Ke Yida
Arrive the effect similar with photoetching process.
What deserves to be explained is, the metal that the present invention is provided receives a micron preparation method for dendrite oldered array, its innovative point it
One is using the conductive array substrate with orderly conductive array, then prepares metallic dendrite battle array by electro-deposition method
Row.There is no at present and metal is made using orderly conductive array and receive a micron precedent for dendrite array, thus the preparation method belongs to out
Invasive innovation and creation.Confirm through many experiments of inventor, the preparation method is universal method, for major part can be corresponding
In aqueous metal salt, electro-deposition goes out the material of metal simple-substance and is suitable for, and corresponding metal can be obtained and receives the orderly battle array of micron dendrite
Row.The method is pervasive to be in the reason for prepared by numerous metallic dendrites：The orderly conductive array substrate for being adopted can be heavy to electricity
Modulating action is played in ion diffusion, nucleation and crystallization process in product, and experiment finds that metallic dendrite is easy in micron size conductive
Bore edges grow out.Further, electro-deposition operation is carried out in conductive array substrate, receive for obtaining the metal of more preferable quality
Micron dendrite oldered array, also needs Reasonable Regulation And Control voltage, electric current, concentration of electrolyte and the parameter phases such as conductive permutation aperture, pitch-row
Coupling, otherwise can only obtain common micro-nano granules or irregular structure array.The present inventor is obtained through the experiment of a large amount of hardships
Of the invention in electro-deposition operation preferred parameter.Additionally, for ZnO, TiO2Change etc. oxide that can be prepared by electro-deposition etc.
Compound, can also adopt the method that oxide dendrite array structure is obtained in principle, but need to explore electrodeposition condition.
The metal that the present invention is provided is received a micron preparation method for dendrite oldered array and is had the advantages that：
1st, the substrate that be suitable to electro-deposition operation is obtained in that by the method that the present invention is provided first, based on the substrate, can
Metal is obtained by electro-deposition method and receives a micron dendrite oldered array, this is that first passage prepares conductive array substrate power-up deposition
Method obtains metal and receives a micron dendrite oldered array；
2nd, obtained metallic dendrite oldered array shape, thickness, size can be made controllable by electro-deposition；
3rd, the preparation method has a extensive future, for ZnO, TiO2Etc. chemical combination such as the oxides that can be prepared by electro-deposition
Thing can also adopt the method that oxide dendrite array structure is obtained in principle；
4th, preparation process is simple, it is easy to operate, Production Time is short, efficiency high, it is adaptable to industrialized production and application.
Description of the drawings
Fig. 1 is obtained conductive array in order after ultraviolet light exposure in embodiment 1；
Fig. 2 is that obtained silver receives the SEM figures of micron dendrite oldered array after electro-deposition in embodiment 1.
Specific embodiment
In order to be better understood by the purpose of the present invention and meaning, with reference to the accompanying drawings and detailed description the present invention is done
Further instruction.
In following specific embodiments, electro-deposition operation is carried out using standard three electrode electrolyzer, to electrode using gold
Category platinized platinum, reference electrode is using the Ag/AgCl being sealed in saturation KCl solution.It should be noted which kind of electrolyzer is adopted,
And following specific embodiments are not limited to using which kind of material to electrode, reference electrode.
Embodiment 1
S1, prepares conductive array substrate：It is 1 μm that photoetching colloid is uniformly coated to coating thickness on conductor, is placed in 380nm
6s is irradiated under ultraviolet light, carry out baking 30min at 120 DEG C, the conductive array substrate with conduction hole array in order is obtained, leads
Electric bore dia is 5 μm, and pitch of holes is 20 μm；
S2, prepares silver nanoparticle dendrite oldered array：In standard three electrode electrolyzer, with conductive array substrate obtained in S1
For working electrode, it is silver nitrate and table to electrode, to be sealed in the Ag/AgCl in saturation KCl solution as reference electrode with platinized platinum
Used as electrolyte, the consumption of CTAB is the 1% of silver nitrate solution molar concentration to face activating agent CTAB, control voltage is -0.8～
0.2V, by voltammetry conductive array substrate the controllable Electrodeposited Silver nanodendrites in surface, electrodeposition time 5 minutes to 2 is little
When, after taking out conductive array substrate, natural air drying obtains silver nanoparticle dendrite oldered array.
Gained silver nanoparticle dendrite is dendritic structure, and size is 50nm～20 μm.
Embodiment 2
S1, prepares conductive array substrate：Photoetching colloid is uniformly coated to conductor, coating thickness is 2 μm, is placed in
3s being irradiated under 220nm ultraviolet lights, carrying out baking 50min at 70 DEG C, the conductive array base with conduction hole array in order is obtained
Bottom, conductive hole are a diameter of 2 μm, and pitch of holes is 10 μm.
S2, prepares gold nano dendrite oldered array：In standard three electrode electrolyzer, with conductive array substrate obtained in S1
For working electrode, it is the chlorauric acid solution to electrode, to be sealed in the Ag/AgCl in saturation KCl solution as reference electrode with platinized platinum
And surfactant SDS is used as electrolyte, the consumption of SDS is the 0.5% of chlorauric acid solution molar concentration, control voltage is -1～
0.5V, by voltammetry conductive array substrate the controllable electro-deposition gold nano dendrite in surface, electrodeposition time 10 minutes to 6 is little
When, after taking out conductive array substrate, natural air drying obtains gold nano dendrite oldered array.
Gained gold nano dendrite is dendritic structure, and size is 25nm～35 μm.
Embodiment 3
S1, prepares conductive array substrate：Photoetching colloid is uniformly coated to conductor, coating thickness is 0.5 μm, is placed in
4min being irradiated under 300nm ultraviolet lights, carrying out baking 10min at 90 DEG C, the conductive array with conduction hole array in order is obtained
Substrate, conductive hole are a diameter of 2.5 μm, and pitch of holes is 15 μm.
S2, prepares copper nanodendrites oldered array：In standard three electrode electrolyzer, with conductive array substrate obtained in S1
For working electrode, it is Schweinfurt green and network to electrode, to be sealed in the Ag/AgCl in saturation KCl solution as reference electrode with platinized platinum
Used as electrolyte, the consumption of EDTA is the 0.2% of acetic acid copper solution molar concentration to mixture EDTA, and control voltage is -3～-0.2V,
By voltammetry conductive array substrate the controllable acid copper nanodendrites in surface, electrodeposition time took for 2 minutes to 10 hours
After going out conductive array substrate, natural air drying obtains copper nanodendrites oldered array.
Gained copper nanodendrites are dendritic structure, and size is 15nm～25 μm.
Embodiment 4
S1, prepares conductive array substrate：Positive-tone photo colloid is uniformly coated to conductor, coating thickness is 5 μm, is placed in
4.5min being irradiated under 360nm ultraviolet lights, carrying out baking 40min at 180 DEG C, the conductive battle array with conduction hole array in order is obtained
Row substrate, conductive hole are a diameter of 10 μm, and pitch of holes is 30 μm；
S2, prepares platinum nanodendrites oldered array：In standard three electrode electrolyzer, with conductive array substrate obtained in S1
For working electrode, it is that potassium chloroplatinate is made to electrode, to be sealed in the Ag/AgCl in saturation KCl solution as reference electrode with platinized platinum
For electrolyte, control voltage is -5～0.5V, by voltammetry conductive array substrate the controllable platinum electrodeposition nanometer branch in surface
Crystalline substance, electrodeposition time 1 minute to 8 hours, after taking out conductive array substrate, natural air drying obtains platinum nanodendrites oldered array.
Gained platinum nanodendrites are dendritic structure, and size is 18nm～40 μm.
Embodiment 5
S1, prepares conductive array substrate：Positive-tone photo colloid is uniformly coated to conductor, coating thickness is 0.9 μm, puts
3min is irradiated under 240nm ultraviolet lights, carry out baking 15min at 220 DEG C, the prepared orderly conductive array with conductive hole
Conductive array substrate, conductive hole are a diameter of 5 μm, and pitch of holes is 30 μm；
S2, prepares ferrum nanodendrites oldered array：In standard three electrode electrolyzer, with conductive array substrate obtained in S1
For working electrode, with platinized platinum be to electrode, to be sealed in the Ag/AgCl in saturation KCl solution as reference electrode, ferrous sulfate and
Used as electrolyte, the consumption of PVP is the 1% of copperas solution molar concentration to surfactant PVP, control voltage is -5～-
0.5V, by voltammetry conductive array substrate the controllable Electrodeposition Bath of Iron nanodendrites in surface, electrodeposition time 3 minutes to 6 is little
When, after taking out conductive array substrate, natural air drying obtains ferrum nanodendrites oldered array.
Gained ferrum nanodendrites are dendritic structure, and size is 22nm～35 μm.
As shown in figure 1, the orderly conductive array substrate obtained after exposing for step S1 ultraviolet light in embodiment 1, from
It can be seen that in coating positive photoresist and after ultraviolet photoetching, orderly conductive array can be obtained in figure.
As shown in Fig. 2 the metal for obtaining after step S2 electro-deposition operation in embodiment 1 receives micron dendrite oldered array
SEM schemes, it can be seen that the metal that the preparation method provided by the present invention is obtained is received micron dendrite and obtains very orderly growth.
The present invention passes through to coat photoresist in conductive substrates, obtains conduction battle array in order through the step such as exposure of ultraviolet light
Row, then after simple electro-deposition, prepare the controllable metal of shape, size, thickness and receive a micron dendrite oldered array.The behaviour
Make method, step is simple, operability and controllability are strong, and popularization in the field of business is obtained.
One of ordinary skill in the art will be appreciated that embodiment described here is to aid in reader and understands this
Bright principle, it should be understood that protection scope of the present invention is not limited to such especially statement and embodiment.This area
It is each that those of ordinary skill can make other without departing from essence of the invention various according to these technology enlightenment disclosed by the invention
Plant concrete deformation and combine, these deformations and combination are still within the scope of the present invention.
Claims (7)
1. a kind of metal receives a micron preparation method for dendrite oldered array, it is characterised in that：With conductive array substrate as work electricity
Pole, electrolyte include that metal salt solution and consumption are additive of the metal salt solution by molar concentration meter 0～5%, by volt-ampere
Method receives a micron dendrite in the controllable electrodeposit metals in its surface, obtains metal and receives a micron dendrite oldered array, the conductive array base
Bottom is the substrate with orderly conductive array, and the additive includes chelating agent or at least one in surfactant, and which is used
In promote metal receive micron dendrite formation and regulate and control pattern.
2. metal according to claim 1 receives a micron preparation method for dendrite oldered array, it is characterised in that：Described orderly
Conductive array, conductive hole are a diameter of 0.1～10 μm, and conductive pitch of holes is a conductive hole aperture between 100 μm.
3. metal according to claim 1 receives a micron preparation method for dendrite oldered array, it is characterised in that：The metal
Micron dendrite of receiving is metal dendritic structure, and size is 10nm～100 μm.
4. metal according to claim 1 receives a micron preparation method for dendrite oldered array, it is characterised in that：The conduction
The preparation method of array substrate is photoetching process, microcontact printing techniques or dip-pen nano process technology.
5. metal according to claim 4 receives a micron preparation method for dendrite oldered array, it is characterised in that：It is based on photoetching
Technique prepares conductive array substrate, specifically includes following steps：
S1, prepares conductive array substrate：Photoresist is uniformly coated to substrate, coating thickness is 0.1～20 μm, is placed in ultraviolet
Toast after irradiating under light, the conductive array substrate with orderly conductive array is obtained；
S2, prepares metal and receives a micron dendrite oldered array：With conductive array substrate obtained in S1, as working electrode, electrolyte includes
Metal salt solution and consumption for the 0～5% of metal salt solution molar concentration additive, by voltammetry in its surface controllable electric
Deposited metal receives a micron dendrite, obtains metal and receives a micron dendrite oldered array.
6. metal receives a micron preparation method for dendrite oldered array according to claim 1 or 5, it is characterised in that：Described
Electrodeposition condition is：- 5～10V of applied voltage, electro-deposition set metallic dendrite size to generation；After the completion of electro-deposition, by conduction
Array substrate is removed, and natural air drying is dried and obtains metal and receive a micron dendrite oldered array.
7. metal according to claim 6 receives a micron preparation method for dendrite oldered array, it is characterised in that：Electro-deposition bar
Part is：Electrodeposition time 10s～10h.
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| CN110299513A (en) * | 2019-06-26 | 2019-10-01 | 中南大学 | A kind of preparation method, parent's lithium cathode and the lithium battery of parent's lithium cathode |
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| CN112630151A (en) * | 2020-12-18 | 2021-04-09 | 成都子之源绿能科技有限公司 | SERS substrate, preparation method thereof and method for measuring pesticide residues by SERS |
| CN113481552A (en) * | 2021-07-14 | 2021-10-08 | 武汉大学 | Preparation method of copper dendrite |
| CN113481552B (en) * | 2021-07-14 | 2022-03-04 | 武汉大学 | Preparation method of copper dendrite |
| CN114525483A (en) * | 2021-12-31 | 2022-05-24 | 安徽大学 | Gold nano dendrite and preparation method and application thereof |
| CN114525483B (en) * | 2021-12-31 | 2023-09-22 | 安徽大学 | Gold nano tree dendrite and preparation method and application thereof |
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